Process for the combined solvent and destructive distillation treatment of oil containing earthy material



Mar. 6, 19-23.

DAY

PROCESS FOR THE COMBINED SOLVENT AND DESTRUGTIVE DISTILLATION TREATMENTOF OIL CONTAINING EARTH! MATHIIAL Filed Aug. 30, 1922 2 sheets-sheet lgmento'z D. T. DAY

PROCESS FOR THE COMBINED SOLVENT AND DESTRUCTIVE DISTILLATION Mar. 6,1923. 1,447,29?

TREATMENT OF OIL CONTAINING EARTHY MATEEIAL Filed Aug. 50, 1922 2sheets-sheet 2 Patented Man-.6, 1923. Q

um'rso PAT-Eur OFFICE; I

DAVID T. DAY, OF WASHINGTON, DISTRICT DECOLUMBIA.

raocrss roa THE comaman SOLVENT am) nasrauc'rrvn msrrua'rron ram'rmn'ror OIL CONTAINING EARTHY MATERIAL. 1 E

' Original application filed December 7, 1820, Serial Ho. 428,913.Divided and thi application fild Aust 80, 1922. Serial No. 585,174.

To whom it may concern: subjected to distillation and this is probablyBe it known that I, DAVID T. DAY, a citi-. due to the fact that dryshale is an extremely pen of the United States, residin at Washpoorconductor of heat and consequently dislngton, in the Dlstrict ofColumbla, have intillation of shale must be not only slow but 5 ventedcertain new and useful Improvewasteful becauseof the time and fuel usedments in Processes for the Combined Solventfor completing thedistillation. Contrasted and Destructive Distillation Treatment of tothe treatment of dry shale, the present Oil Containing Earthy Material,of which process, by treating oil soaked shale, and the following is aspecification. particularly shale soaked with hot oil,

'10 This invention relates to a process for efshortens the requiredperiod of heating befecting the extraction of oil from oil bearcause ofthe initial rise in temperature due ing shale, and earthy material, suchas sand, to the presence of hot oil extending into the and provides forextraction with a liquid center of each particle of shale and the factbath of solvent combined with destructive that oil soaked shale is abetter conductor of 4 l5 distillation. heat than the same shale in adrier condi- The invention provides specifically the tion. process inwhich a bath or pool of li uid Apparatus'in which the process may besolvent is used and into which fresh s ale conducted should include aretort for the is passed, the partial extraction of the oil distillationof the shale which has been pre- 20 from the earthy material by thesolvent, the viously oil soaked, a treatment chamber for removal of theearthy material from the subjecting untreated shale to a bath of hotbath of oil, and the subsequent distillation of liquid oil, andcommunicating pipes providthe earthy material so removed to effect ingfor the passage of the products of distilcracking of the oil therein andthe produclation from the retort to a point where these 25 tion of oilfor the maintenance of the oil products may be conveniently condensed toa bath. suflicient degree to provide the materials The process has madeit possible to obused as the liquid bath in the treatment tain a largertotal yield of oil than is ordichamber. Details providing for theefficient narily possible by either the usual solvent and continuousoperation of the process may 30 extraction or by destructivedistillation. also include the use of a screw, chain type,

Solvent extraction may remove three times or any other suitable type ofconveyor retort as much oil from shale as is possible by depositionedsubstantially -vhorizontally in a structive distillation. The presentinvenfurnace, an inclined tubular treatment chamtion combines thesolvent features with disber above the retort tube and outside the'tillation in a way that uses the products furnace, and the relativeposition of the formed during distillation to serve as maopenings forthe introduction and removal terial for the solvent bath. of shale orother solid or earthy material, the The advantageous results" madepossible relative position of the pipes for the removal by the inventionare due also in part to the of liquid oil and aeriform material fromthe40 heat exchange wherein the heat of condensatreatment chamber, therelative length of the tion of the va ors within the solvent extracpipesconnected to the treatment chamber,

tion chamber heats the earthy material asit and the mounting of aconveyor within the moves through the chamber and thus enables treatmentchamber for the removal of shale. the earthy material to go into theretort at Claims directed to the distinctive apparatus a temperatureequal to the boiling point of features are presented in my applicationthe solvent. Another feature provided by Serial No. 428,913 filedDecember 7, 19.20,

the use of very hot oil on the earthy mafrom which this application hasbeen diterial is the advantage derived by the invided.

creased ease and rapidity with which the oil The above and additionaldetails and ad- 50 soaked earthy material is treated in a retortvantages of the process are described and,

to destructive distillation. In the treatment claimed in the followingspecification and of shale, the process has been found to opclaims.Apparatus for conducting the crate much more readily than was the caseprocess is illustrated in the accompanying where relatively dry ilbearing shale was drawings, in which; Y

' treatment chamber positioned above the retort; and

Figure 3 is a diagrammatic view illustrating the relative direction ofrotation of the conveyor shafts, looking in the directlon of the arrowson-the line 3-3 of Figure 2.

Like numerals refer to like parts in the different figures of thedrawing.

Referring in detail to the drawings of the apparatus which has beensuccessfully used in conducting the process of the invention, 1represents the masonry constructed of the furnace, either concrete,stone or brick, but preferably firebrick, such as will stand severtemperatures. A suitable stack 2 is provided for leading off the furnacefumes, smoke, and gases of combustion. A source of heat is provided byburners 3 located at the lower part of the furnace and fed by suitablepipes 3 providing liquid or gaseous fuel obtained during the operationof the process and apparatus, as will be hereinafter further explained.The furnace may be braced by suitable buck stays, not shown, whichenclose the outer walls of the furnace and hold the same to a suitablemasonry or concrete base. The flame and hot gases from the burnernozzles is projected inwardly and passed upwardlyin the furnace over ahorizontally extending partition 4 and upward to ultimately escapethrough the stack 2. Durino the upward movement the heat comes intodirect contact with the exterior of a plurality of longitudinallypositioned retort tubes, as will be described.

The drawing illustrates three cracking tubes or retort tubes 5, 6 and 7,positioned one above the other and substantially horizontally. Withinthe tubes 5, 6 and 7 are respective screw conveyors 5 6 and 7, mountedon and adapted to turn with shafts 5", 6 and 7, respectively. Suitablejournal boxes or stufiing boxes are indicated for respective shafts at5, 6 and 7". Materials within the tube 5 are passed to the left,referring to Figure 2, and are dropped through the communicating pipe 8into the end of the tube 6, and similarly these materials are passed inthe opposite direction in the tube 6 and are permitted to drop throughthe communicating pipe 9 to the lowermost tube 7, in which latter thematerials are again moved to the left and are finally dropped into thedischarge pipe 10 for spent shale. Discharge pipe 10 has a rotary valve10 adapted to periodically move to discharge shale in measured quanmeme? tities, but not to permit the passage of air or gases into or outof the retort. The-valve 10 is mounted on a shaft 10 and operated by thesame power means as the shafts of the retort conve ors, as will bedescribed. The direction 0 travel of the contents .of the apparatus isindicated by arrows.

Immediately above the retort and furnace is mounted a treatment chamber11 adapted to contain a 001 or bath of liquid oil. Th1s chamber is ilustrated as an. inclined tubular longitudinally extending member havingits lower end adjacent the outlet end of the retort and its upper endpositioned above the inlet end of the upper retort tube 5. A pipe 12 isindicated on the upper side of and lead-.

ing from an opening in the chamber 11 adjacent the lower end thereof andcommunicat'es with a reservoir 13 above the same, which reservoir isprovided with a suitable funnel shaped opening 14. At the opposite andupper end of the chamber 11 and on the underneath side thereof is adischarge opening having a pipe 15 leading therefrom and extendindownwardly as a supply pipe for the receiving end of the retort tube 5.A screw conveyor 11 is mounted within the chamber 11 and positionedsubstantially on the bottom thereof so as to move shale and solidmaterial along the inclined floor of the chamber from the lower endthereof and dump such material into the pipe 15. The screw conveyor 11*-is mounted on shaft 11 which in turn is provided with the necessarystufling boxes or journal boxes 11 at the ends of the chamber 11. Therate of treatment of the solid material is comparatively I tively slowlyfrom the lower.end of the chamber 11 to the discharge opening at thepipe 15. In addition to the rate of treatment, the invention alsoprovides for the soaking of the oil by providing that the lower end ofthe chamber 11 constantly contain a bath or pool of liquid oil whichnormally covers the lower end of the pipe 12 and rises within that pipeand into the hopper 13 whenever the pressure may so require thismovement. Likewise it is necessary that the upper end of the pipe 15,namely the discharge end of the chamber, be above the fluid level withinthe chamber so that the screw conveyor 11' may move shale material outof the liquid oil bath before dumping the shale material into the pip15. On the upper side of the chamber is a discharge arrangement thispipe is in close proximity to the pipe 12 near the upper surface buttoward the lower end of the chamber 11. An

upwardly extending pipe 17 having its upper end open to the air isconnected to the pipe 17 to permit equalization of pressure and toprevent siphoning of oil through the pipe 17 when flow is startedthrough this pipe. The pipe 17 should extend approximately as high asthe upper end of the reservoir 13 so that the oil also may rise withinthis pipe subject to pressures within the chamber 11, as will bedescribed.

The pipe 16 for the removal of aeriform materials preferably extendsupward as an elongated run-back pipe, and is connected with a stonetower 18, and from this tower gases and lighter vapors are removedthrough the pipe 19 and passed through the coils of a condenser 20positioned in the condenser tank 21. Liquid oil formed within the stonetower is drawn off through the pipe 22 and emptied into a distillatetank 23. Materials condensed in the coils 20 are removed through. a pipe20 and deposited in a gasolene tank 24. Gases remaining after passagethrough the condense-r are led upward away from the pipe 20 and into agas scrubber 25 by means of a pipe 20' connected to the lower end of thescrubber. The gases issuing from the scrubber at the top thereof are ledthrough the pipe 3 to the burner nozzle 3 in the furnace. The pipe 17for the removal of liquid oil from the oil bath in the chamber 11,extends the length of the apparatus, back of the con denser in Figure 1,and is connected to the pipe 22 which conducts liquid oil into thedistillate tank 23.

Driving means for turning the shafts 5 6", 7 and 11 is provided by themain drive shaft 26 mounted to suitable bearings, not shown and drivenfrom any suitable source of power. Referring to Figures 2 and 3, it willbe noted that the shaft 26 moves counter clockwise and turns a sprocketgear 27, which in turn operates a continuous chain 28, which latter inturn extends over the sprocket gears 5 6 and 7 d which are mountedrespectively on the conveyor shafts 5 6 and 7". The shaft 5 is providedwith a second sprocket gear 5 which is adapted to drive a chain 5passing over a sprocket gear 11 mounted on the conveyor shaft 11". Auniversal joint in the shaft 11 is indicated at 11 to take care of the"angle due to the inclination of the tank 11. At the lower side of theapparatus the conveyor shaft 7 is provided with a second sprocket wheel7 which drives a chain 7. passing" over a sprocket wheel 10 mounted, nthe valve shaft 10 thus constituting operating means for the valve 10.The arrows in Figure 3 indicate the relative direction of rotation ofthe-conveyor shafts and sprocket wheels.

At the upper end of the treatment chamber 11 is a pipe 11 for theintroduction of materials used for washing out the treatment chamber,and at the lower end is a corresponding drain pipe 11 for removing suchmaterials.

The process has been satisfactorily conducted with apparatus in whichthe retort tubes 5, 6 and 7 were approximately of six inchbore, and inwhich a conveyor screw of five and three-quarter inches was operated.The invention preferably uses a tubular treatment chamber 11 which has abore of from twenty-four to thirty inches in which the conveyor memberis approximately eight inches. The operation of the' process is notnecessarily dependent on the relative size of the chamber and conveyortherein, but under certain conditions ,may be operated satisfactorilywith a conveyor substantially filling the chamber, or by any kind ofequipment capable of moving shale and solid material from the pool ofoil, out of the same, and introducing it into the receiving end of theretort.

In the normal operation of the process, when first starting the same,liquid oil is poured into the opening 14 and sufiicient is introduced tocover the lower end of the pipe 12, thus forming a liquid seal for thispipe. Such oil is preferably a distillate obtained from previousdistillation, or what is known as tops or distillate, but any otherliquid oil from petroleum is sufficiently eifective as a seal to servefor the purpose. The use of water as a seal for the initial operationhas been satisfactorily applied.

Crushed shale or other solid material containing the oil to beextracted, in reduced form and containing chiefly lumps capable ofpassing through a two inch screen, is added by dumping the same in smallamounts into the opening 14. The shale is introduced thus into the oilbath and is sub jected thereby to a combined solvent treatment and oilsoaking treatment. The con veyors are set in motion and the retortheated. It is the practice to introduce shale into a reservoir 13 asfast as it is removed by the screw conveyor 11, thus giving a mechanicaladvantage of preventing an accumulation of the shale, which because partof it is finely divided when stirred up with the oil, becomes amud whichis objectionable when'passed into pipes. The column of shale moved alongthe floor of the chamber llflis relatively small compared to thecapacity of the chamber, usually not more than 10 per cent, as suchshale being present as compared to the volume of the oil bath, andfrequently the amount of shale is in much lower proportion. This continuous movement of the shale in small quantities is such that the shale isconstantly in agitation and being stirred and is in constant contactwith new portions of a relatively large bath of solvent oil. As theshale is moved from the chamber and through the retorts' in the retortfurnace it is subjected to increased temperatures during its progressthrough the apparatus. This heat treatment in the retorts drives off alloil material present in the shale and adhering thereto, and all that hasnot been removed by the solvent action of the bath of oil in the chamber11. The gases and vapors generated within the retort tubes 5, 6 and 7are passed upward through the pipe 15 and into the treatment chamberll.In this region they come into contact with the relatively cooler wallsof the chamber, the bath of oil with the fresh shale therein, and asubstantial portion of the material is condensed and flows to the lowerend of the chamber to supplement the volume of liquid oil. The natureand the amount of the materials so condensed depends on the temperaturein, the retort, in part, but chiefly on the relative size and coolnessof the walls of the treatment chamber 11 and the length of the runbackpipe 16. The chamber 11 may be covered with insulating material tomaintainheat conditions constant, or it may be artificially cooled.Likewise, the length ofthe pipe 16 may be varied and it also maybeinsulated or artificially cooled, such changes depending on the relativenature of the condensed materials tobe used as the'solvent bath.

The blast of flame from theJourners 3 rovides a temperature in thelower-retort hotter than the temperature in the upper retort. Thetemperature around the retort tubes should be from 900 F. to 15100 F.

. depending on the arrangement of flues' and the disposition of theretort tubes within" the furnace 1. The temperature within the retorttubes should be at least 550 F and for the practical rapid operationabout 700 F. is desired. However, the temperature within the tube doesnot have to be as high as ordinarily used for destructive distillationin small retorts, because in the present invention the heat istransmitted with comparative rapidity from the outside to the inside ofeach piece of shale, this being due, as hereinbefore explained, to thepreliminary heating by the addition of the hot solvent oil whichthoroughly soaks each piece of shale and'likewise raises the temperatureof the same. The product is im proved because of the cracking whichtakes place within the lumps of shale, this particular cracking beingimproved by the presence of the shale itself. The temperature within theextraction chamber 11 is subs'tantially the same as the temperature ofthe vapors issuing from the retort tubes through the pipe 15, as theyare condensed to form the li uid of the extracting bath:

These vapors t us condensed are approximately at a temperature of 300F., and sometimes above, and sometimes below, depending on the positionof the chamber 11 relative to the outside air, the distance from thefurnace, and the constant cooling effected by such conditions.

The process is capable of operation at ordinary atmospheric pressure,under partial vacuum, and also under increased pressure. In the ordinaryoperation, the liquid'oil in the lower end of the chamber 11, bycovering the lower end of the pipe 12, merely provides a liquid seal andempties out through the pipe 17, flowing to the distillate tank 23,

and no pressure different from atmospheric pressure is used. A gain inefiiciency has been obtained when pressures up to 70 pounds at leasthavebeen ap lied, and under increased pressure extractlon takes place morerapidly and completely on account of the higher temperature at which thesolvent remains liquid instead of vaporizing. Pressures may be built upby partially closing the valves in the pipes 16 and 17, and the pipe 12and the reservoir 13, it also rises -in the air vent pipe 17, whichlatter should be high enough to permit this rise in liquid level.

The liquid oil taken off through the pipe 17 from the liquid extractionbath in the 0 lower end of chamber 11 differs from theliquid obtainedfrom the vapors which passofi' through the pipe 16, because the. formercontains more or less of dissolved material extracted from the shale.The liquid in the chamber 11 alsocontains a more readily condensed vaporpassed from the retort, and therefore has a higher specific gravity andhigher boiling point than the vapors and the liquids condensed therefromwhich are driven ofi' through the pipe 16. a

The process has been successfully conducted in the treatment ofMonterey, shale mined in California. Also, it has been successfully usedin treating shales mined near Elko, Nevada, which latter containdargeamounts of oil and wax which can be extracted by solvents. The inventionhas. also been successfully used with shale taken from the Uintah Basinof Colorado and Utah, and also has successfully been used with oilsoaked sand.

The process has produced remarkable results by using the steps ofoperation and the details hereinbefore spec-ified. These featuresinclude the use of materials extracted by distillation as the materialof a solvent bat-h for treating shale. Other arrangements capable ofperforming the steps specified for the process may be possible, but sucharrangements are considered as within the scope of the process of thisinvention. For instance, the treatment chamber could extend downwardfrom the right of the furnace so as to lower the chamber and in thiscase the upper end of the treatment chamher would have the same relativeposition as regards the connecting pipe 15, but the lower end of thechamber would be nearer the ground and consequently the reservoir 13would be more readily reached. This arrangement might serve also toextend the lower end of the treatment chamber toward the source of shalesupply thereby reducing the amount of conveyor apparatus necessary. Theapparatus arrangement illustrated with the, treatment chamber above theretort serves to economize fioor space although the upper end of thereservoir 13 may not be as easily reached as if the treat.- ment chamberwas inclined downwardly toward the ground and positioned at one side ofthe furnace.

The term hydrocarbon oil material is understood to include all materialremovable from the shale by the process described and" which bedscontain such resin, also contains in solution. amounts of resin andallied oxidized bodies such as tar and wax, and that this material maybe recovered and separated by treating the oil as it is obtained fromthe ground. The presence of such materials in solution in oil in natureindicates the correctness of the theory of the present invention, whichprovides for the solvent extraction of the shale by the solvent obtainedfrom the shale.

I claim:

1. The process of obtaining hydrocarbon oil material from oil bearingearthy material which process consists of subjecting the earthy materialto be treated to immersion in a bath of liquid oil in a container.separating the earthy material from saidbath of oil, subjecting all ofsaid earthy material so separated to heat treatment to drive of!substantially all volatilizable material therefrom, and passing thematerial thus driven ofi into the container of said bath of oil andutilizing the hydrocarbon material so driven ofi as the material of saidbath of liquid Oll. 2. The process of obtaining hydrocarbon oil materialfrom oil bearing earthy material which process consists of subjectingthe earthy material to be treated to immerslon in a bath of liquid oilin a container, separating the earthy material from said bath of oil,subjecting all of said earthy material so separated to heat treatment todrive oii' substantially all volatilizable material therefrom, passingthe material thus driven off into the container of said bath of oil andutilizing the hydrocarbon material-so driven off as the material of saidbath of liquid oil, and withdrawing liquid oil from sald bath.

3. The process of obtaining hydrocarbon oil material from oil bearinearthy material which process consists oi subjecting the earthy materialto be treated to immersion in a bath of liquid oil in a container,separating the earthy material from said bath of oil, subjecting all ofsaid earthy material so separated to heat treatment to drive offsubstantially all volatilizable material therefrom, passing the materialthus driven off into the container of said bath of oil and utilizing thehydrocarbon material so driven oil as the material of said bath ofliquid oil, and withdrawing aeriform material from the region of saidbath of oil.

4:. The process of obtaining hydrocarbon oil material from oil bearingearthy material which process consists of subjecting the earthy materialto be treated to immersion in a bath of liquid oil in a container,separating the earthy material from said bath of oil, subjecting all ofsaid earthy material so separated to heat treatment to drive offsubstantially all volatilizable material therefrom, passing the materialthus driven ofi into the container of said bath of oil and utilizing thehydrocarbon material so driven off as the material of said bath ofliquid oil. withdrawing liquid oil from said bath, and withdrawingaeriform material from the region of said bath of oil and subjecting theaeriform material to a condensing treatment.

5. The process of continuously obtaining hydrocarbon oil from oilbearing earthy material which procem consists of continuouslysubjecting'the earthy material to be treated to immersion in a bath ofliquid oil in a container, continuously separating all of said earthymaterial soseparated to heat treatment to drive off substantially allVola tilizable material therein and passing the material thus driven offinto the container of said bath of oil and continuously utilizing thehydrocarbon material so driven oit as the material of said bath ofliquid oil.

6. The process of continuously obtaining hydrocarbon oil material fromoil bearing earthy material which process consists of continuouslysubjecting earthy material to continuously subjecting all of said earthymaterial so separated to heat treatment to drive ofi substantially allvolatilizable material therefrom, passing the material thus driven ofiinto the container of said bath of oil and continuously utilizing thehydrocarbon material so driven ofi as the material of said bathof'liquid oil, and continuously withdrawing liquid oil from said bath.

'7. The process of obtaning hydrocarbon oil material from oil bearingearthy material which rocess consists of continuously subjecting t eearthy'material to be treated to immersion in a bath of liquid oil in acontainer, continuously separating the earthy material from said bath ofoil, continuously subjecting all of said earthy material so separated toheat treatment to drive oil substantially all volatilizable materialtherefrom, passin the material thus driven off into the container ofsaid bath of oil and continuously withdrawin aeriform material from theregion of saidath of oil.

8. The process of obtaining hydrocarbon oil material from oil bearingearthy material which process consists of continuously subjecting theearthy material to be treated to immersion in a bath of liquid oil in. acontainer, continuously separating the earthy material from said bath ofoil, continuously subjecting all of said earthy material so separated toheat treatment to drive ofi substantially all volatilizable materialtherefrom, passing the material thus driven off into the container ofsaid bath of oil and continuously utilizing the hydrocarbon material sodriven off as the material of said bath of liquid oil, continuouslywithdrawing liquid f separating the earthy material from said bath ofoil, subjecting all-of said earthy material so separated to heattreatment to drive off substantially all volatilizable hydrocarbonmaterial therefrom, and passing the material thus driven ofi' into thecontainer of said bath of oil and utilizing the hydrocarhon material sodriven off as the material of saidbath of liquid oil.

10. The process of obtaining hydrocarbon oil material from oil bearingearthy material which process consists of subjecting a relatively smallamount of the earthy material to be treated to immersion in a relativelylarge bath of hot liquid oil in a container and permitting said hotliquid oil to permeate the earthy material, separating the earthymaterial from said bath of oil, subjecting all of said earthy materialso sepa rated to heat treatment to drive oil substantially allvolatilizable hydrocarbon material therefrom, and passing the materialthus driven off into the container of said bath of oil and utilizing thehydrocarbon material so driven off as the material of said bath ofliquid oil.

11. The process of obtaining hydrocarbon oil material from oil bearingearthy material which process consists of subjecting the earthy materialto be treated to immersion in a bath of solvent liquid oil to efi'ectthe solvent removal from said earthy material of a portion of its oilcontent, separating the earthy material from said bath of oil,subjecting the earthy material so separated to heat treatment to driveoff substantially all volatilizable material therefrom, and utilizingthe hydrocarbon material so driven off as1 the material of said bath ofsolvent liquid 01 12. The process of obtaining hydrocarbon oil materialfrom oil bearin earthy material which process consists of subjecting theearthy material to be treated to immersion in a bath of solvent liquidoil to effect the solvent removal from said earthy material of a portionof its oil content, separating the earthy material from said bath ofoil, subjecting the earthy material so separated to heat treatmentsuflicient to drive off substantially all volatilizable materialtherefrom and crack a portion of the same, and utilizing the hydrocarbonmaterial so driven off aslthe material of said bath of solvent liquid or13. The process of obtaining hydrocarbon oil material from oil bearinearthy material which process consists 0 subjecting the earthy materialto be treated to immersion in a. bath of solvent liquid oil to effectthe solvent removal from said earthy material of a portion of its oilcontent, separating the earthy material from said bath of oil,subjecting the earthy material so separated to heat treatment suflicientto drive off substantially all volatilizable material therefrom andcrack a portion of the same,-and utilizing the hydrocarbon material sodriven off at a temperature of at least 300 F. as the material of saidbath of solvent liquid oil.

In testimony whereof I afiix my signature.

DAVID T. DAY.

